反应详情

To refluxing acetic anhydride (1050 g., 10 moles), there is added dropwise over six hours a solution of camphene (136 g., 1 mole) and di-tert-butyl peroxide (0.1 mole, 14.6 g.). After complete addition, the mixture is heated at reflux for five hours. The cooled reaction mixture is concentrated under reduced pressure to leave a yellow-orange residual oil; 750 ml. of 2.5N NaOH is added to the residue which is then heated on the steam bath for one hour. The cooled solution is extracted once with ether, made acidic with concentrated HCl, and extracted thoroughly with ether. The dried (Na2SO4) ether extracts are concentrated under reduced pressure and the residue distilled under vacuum to give a colorless product, b.p. 141° C.-144° C./0.5 mm.

1. additionAfter complete addition
2. temperaturethe mixture is heated
3. temperatureat reflux for five hours
4. customThe cooled reaction mixture
5. concentrationis concentrated under reduced pressure
6. customto leave a yellow-orange residual oil
7. temperatureis then heated on the steam bath for one hour
8. extractionThe cooled solution is extracted once with ether
9. extractionextracted thoroughly with ether
10. dry with materialThe dried (Na2SO4) ether extracts
11. concentrationare concentrated under reduced pressure
12. distillationthe residue distilled under vacuum
13. customto give a colorless product, b.p. 141° C.-144° C./0.5 mm